CN108318612B - Method for determining content of silver impurities in MOX (metal oxide x) pellet by using TBP (tert-butyl phosphate) extraction resin - Google Patents

Method for determining content of silver impurities in MOX (metal oxide x) pellet by using TBP (tert-butyl phosphate) extraction resin Download PDF

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CN108318612B
CN108318612B CN201711448396.6A CN201711448396A CN108318612B CN 108318612 B CN108318612 B CN 108318612B CN 201711448396 A CN201711448396 A CN 201711448396A CN 108318612 B CN108318612 B CN 108318612B
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梅家文
张庆桂
张永红
朱宙林
高娟
王跃龙
代亚会
敖亚丽
李艳平
杨军梅
吴金德
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404 Co Ltd China National Nuclear Corp
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Abstract

The invention relates to the technical field of fuel detection, and particularly discloses a method for determining the content of silver impurities in an MOX pellet by using TBP extraction resin, which comprises the following steps: step 1: processing a sample; step 2: preparing an instrument; and step 3: drawing a working standard curve; and 4, step 4: testing a sample; and 5: and (6) calculating a result. The invention realizes the rapid and accurate determination of the content of the silver impurity element in the MOX pellet, the lower limit of the determination method of the content of the silver impurity element is 0.9 mug/g under the condition that the sample amount is 0.100g, the measurement precision is better than 5 percent, and the recovery rate of the method is 92 to 107 percent.

Description

Method for determining content of silver impurities in MOX (metal oxide x) pellet by using TBP (tert-butyl phosphate) extraction resin
Technical Field
The invention belongs to the technical field of fuel detection, and particularly relates to a method for determining the content of silver impurities in an MOX pellet by using TBP extraction resin.
Background
The experimental fast reactor mixed uranium plutonium oxide fuel (MOX) pellet in China needs to carry out limit control on the content of 18 impurity elements such as aluminum, silver, calcium, copper and other elements, the content of each impurity element needs to be monitored in each link of pellet manufacturing, and the silver impurity element is an important control index of the MOX pellet.
At present, an analysis method for impurity elements such as silver in MOX pellets is not established in China. The standard for determining the silver content of mixed uranium plutonium oxides is ASTM C698-2010 Nuclear grade Mixed uranium plutonium oxide ((U, Pu) O)2) The standard test method for chemical, mass and spectrochemical analysis of (1)', the determination method is carrier distillation spectrometry, which is to grind a sample into powder and then put the powder into a graphite electrode, record the characteristic spectrum excited by each element in a spectrograph under the excitation of a direct current power supply by using a photosensitive phase plate, measure the blackness value by using a micrometer photometer after the photosensitive phase plate is developed, calculate the content of each element through an emulsion calibration curve and an analysis curve, and have the measurement precision only superior to 25 percent. If a proper sample preparation method and an appropriate sample preparation instrument are adopted, the method for measuring the content of the impurity elements by using the ICP-AES in the standard C1432 can replace the carrier distillation spectrometry in the C698-2010, but the 25 impurity elements measured by the method for measuring the content of the impurity elements by using the ICP-AES in the C1432 do not contain silver elements.
At present, ICP-AES is widely used for measuring trace elements in various materials and has the characteristics of wide linear range, high accuracy, high analysis speed and the like. But is limited by the particularity of radioactive material detection, and the technology for measuring the silver content in the MOX pellet by adopting TBP extraction resin separation-ICP-AES is not published and reported in public.
Disclosure of Invention
The invention aims to provide a method for determining the content of silver impurities in an MOX pellet by using TBP extraction resin, which can accurately and quickly determine the content of trace silver impurity elements in the MOX pellet.
The technical scheme of the invention is as follows:
a method for determining the content of silver impurities in an MOX pellet by using TBP extraction resin comprises the following steps:
step 1: sample processing
1.1 sample dissolution
Grinding the MOX pellets into powder with the particle size of less than 150 mu m, weighing 100mg of MOX pellet powder into a polytetrafluoroethylene crucible, and adding 1-4 m L concentrated HNO containing 0.1 mol/L hydrofluoric acid3Dissolving with mixed acid;
after the sample is completely dissolved, 0.5m L6 mol/L nitric acid solution is added, the mixture is slowly heated and steamed on an electric furnace till the mixture is nearly dry, and then 1m L6 mol/L nitric acid solution and H are added2O2Adjusting the valence, after the plutonium is adjusted to 4 valence and the uranium is adjusted to 6 valence, heating to drive out H2O2Concentrating to near dryness, adding 0.5m L6 mol/L mol nitric acid for dissolution and separation;
1.2 chromatographic column preparation
Pouring TBP extraction resin slurry into a quartz chromatographic column filled with deionized water, uniformly loading by using a stirring rod, removing bubbles by light pressure, cleaning the filled chromatographic column by using a 0.1 mol/L nitric acid solution, removing impurities, then washing by using deionized water until the chromatographic column is neutral for later use, and carrying out balance treatment by using a 5-10 m L6 mol/L nitric acid solution before use;
1.3 sample isolation
Transferring the sample solution into a well-balanced TBP extraction resin chromatographic column, then leaching with 7-9 m L6 mol/L nitric acid solution at the leaching speed of 0.2-0.5 m L/min, receiving the leacheate into a 10m L quartz volumetric flask, and fixing the volume to the scale with 6 mol/L nitric acid solution to be used as a solution to be measured;
1.4 blank solution preparation
Preparing a blank solution for the same batch of samples according to the step 1.1-step 1.3;
step 2: instrument preparation
Preheating the ICP spectrometer for more than 60min after starting up, and stabilizing plasma for 15-30 min after ignition;
setting method parameters in software, selecting a silver element analysis spectral line at 328.0nm, and setting the working conditions that the carrier gas flow is 0.5L/min, the RF power is 900W, the sample lifting amount is 1.4L/min, and the auxiliary gas flow is 1.0L/min;
and step 3: drawing working standard curve
Using a 6 mol/L nitric acid solution as a blank standard solution, diluting a silver standard stock solution with the 6 mol/L nitric acid solution to prepare a working standard solution of 1 mu g/m L, introducing the blank standard solution and the working standard solution into an ICP spectrometer in sequence for measurement, and automatically drawing a working standard curve by the instrument;
and 4, step 4: sample assay
The blank solution and the sample solution to be measured are sequentially put into an ICP spectrometer for measurement, and the instrument automatically calculates the blank concentration value rho of the silver impurity element0And sample solution concentration value ρi；
And 5: calculation of results
Calculating the content of silver impurity elements in the MOX pellet sample according to the formula (1):
Figure GDA0002403968830000031
in the formula:
wi-the content of silver impurity elements in the sample, μ g/g;
ρi-the concentration value of silver impurity element in the sample solution, μ g/m L;
ρ0-the concentration value of silver impurity elements in the blank solution, μ g/m L;
v — volume of sample solution, m L;
m represents the sample weighing amount and g.
When parallel measurement is carried out on the samples of the same batch and a single sample, the step 2 and the step 3 are not repeated.
In the step 1.2, the TBP extraction resin is 150-200 meshes, and 60% of TBP is contained in the TBP extraction resin.
In the step 1.2, the inner diameter of the quartz chromatographic column is 6mm, the height of the quartz chromatographic column is 200mm, the height of the quartz chromatographic column is 150mm, and the bottom of the quartz chromatographic column is filled with glass wool.
Step 1.3, when the sample solution is transferred into the well-balanced TBP extraction resin chromatographic column, the first 0.3m L effluent liquid is discarded.
And 3, preparing the silver standard stock solution from a certified standard substance GSB G62039-90.
And 5, carrying out data calculation according to GB/T8170 to carry out reduction, wherein the analysis result is less than 10, one decimal is reserved, the analysis result is more than or equal to 10, and the decimal is not reserved.
In step 1, the MOX pellet powder is weighed to be accurate to 0.0001 g.
The ICP spectrometer can be in butt joint with the enclosed glove box.
The ICP spectrometer is an IRIS Integrated II type full spectrum direct reading plasma spectrometer produced by ICP-AES, United states thermoelectricity company.
The invention has the following remarkable effects:
the invention realizes the rapid and accurate determination of the content of the silver impurity element in the MOX pellet, the lower limit of the determination method of the content of the silver impurity element is 0.9 mug/g under the condition that the sample amount is 0.100g, the measurement precision is better than 5 percent, and the recovery rate of the method is 92 to 107 percent.
Drawings
FIG. 1 is a schematic flow chart of a method for determining the content of silver impurities in an MOX pellet by using TBP extraction resin.
Detailed Description
The invention is described in further detail below with reference to the figures and the embodiments.
A method for determining the content of silver impurities in an MOX pellet by using TBP extraction resin comprises the following steps:
step 1: sample processing
1.1 sample dissolution
Grinding the MOX pellets into powder with the particle size of less than 150 mu m, weighing 100mg of MOX pellet powder to be accurate to 0.0001g, and adding 0 in a 1-4 m L polytetrafluoroethylene crucible with the particle size of 50m L.Concentrated HNO of 1 mol/L hydrofluoric acid3Dissolving with mixed acid, adding 0.5m L6 mol/L nitric acid solution after sample is completely dissolved, slowly heating and steaming on electric furnace to near dryness, adding 1m L6 mol/L nitric acid solution and H2O2Adjusting the valence, after the plutonium is adjusted to 4 valence and the uranium is adjusted to 6 valence, heating to drive out H2O2Concentrating to near dryness, adding 0.5m L6 mol/L mol nitric acid for dissolution and separation;
1.2 chromatographic column preparation
Pouring TBP extraction resin slurry into a quartz chromatographic column filled with deionized water, uniformly loading by using a stirring rod, removing bubbles by light pressure, cleaning the filled chromatographic column by using a 0.1 mol/L nitric acid solution, removing impurities, then washing by using deionized water until the chromatographic column is neutral for later use, and carrying out balance treatment by using a 5-10 m L6 mol/L nitric acid solution before use;
the TBP extraction resin is 150-200 meshes and contains 60% of TBP; the quartz chromatographic column has an inner diameter of 6mm, a height of 200mm, a column height of 150mm and a column bottom pad of glass wool.
1.3 sample isolation
Transferring the sample solution into a well-balanced TBP extraction resin chromatographic column, discarding the front 0.3m L effluent liquid, then leaching with 7-9 m L6 mol/L nitric acid solution at the leaching speed of 0.2-0.5 m L/min, receiving the leaching solution into a 10m L quartz volumetric flask, and fixing the volume to the scale with 6 mol/L nitric acid solution to be used as a solution to be measured;
1.4 blank solution preparation
A blank solution is prepared for the same batch of samples according to steps 1.1-1.3.
Step 2: instrument preparation
Preheating the ICP spectrometer for more than 60min after starting up, and stabilizing plasma for 15-30 min after ignition;
the method parameters are set in the software, the silver element analysis spectral line is selected to be 328.0nm, and the working conditions are set to be that the carrier gas flow is 0.5L/min, the RF power is 900W, the sample lifting amount is 1.4L/min, and the auxiliary gas flow is 1.0L/min.
And step 3: drawing working standard curve
The method comprises the steps of using a 6 mol/L nitric acid solution as a blank standard solution, diluting a silver standard stock solution with a 6 mol/L nitric acid solution to prepare a working standard solution with the concentration of 1 mu G/m L, sequentially introducing the blank standard solution and the working standard solution into ICP-AES for measurement, and automatically drawing a working standard curve by an instrument, wherein the silver standard stock solution is a certified standard substance GSB G62039-90.
And 4, step 4: sample assay
The blank solution and the sample solution to be measured are sequentially put into an ICP spectrometer for measurement, and the instrument automatically calculates the blank concentration value rho of the silver impurity element0And sample solution concentration value ρi。
And 5: calculation of results
Calculating the content of silver impurity elements in the MOX pellet sample according to the formula (1):
Figure GDA0002403968830000061
in the formula:
wi-the content of silver impurity elements in the sample, μ g/g;
ρi-the concentration value of silver impurity element in the sample solution, μ g/m L;
ρ0-the concentration value of silver impurity elements in the blank solution, μ g/m L;
v — volume of sample solution, m L;
m represents the sample weighing amount and g.
And (3) carrying out data calculation according to GB/T8170, wherein the analysis result is less than 10, one decimal is reserved, the analysis result is more than or equal to 10, and the decimal is not reserved.
When parallel measurement is carried out on the samples of the same batch and a single sample, the step 2 and the step 3 are not repeated.
The ICP-AES used by the invention is an IRIS Intrepid II type full spectrum direct reading plasma spectrometer produced by the United states of America thermoelectric company, and other ICP spectrometers in the market can also be suitable for the invention if the ICP-AES is in butt joint with an enclosed glove box.
Example one
Step 1: treatment of blank solution
1.1 blank solution preparation
4m of L concentrated HNO containing 0.1 mol/L of hydrofluoric acid was added to a 50m L Teflon crucible3Mixing the acid, steaming to near dryness, adding 0.5m L6 mol/L nitric acid solution, slowly heating on an electric furnace, steaming to near dryness, adding 1m L6 mol/L nitric acid solution and H2O2Then heating to drive off H2O2Concentrating to near dryness, adding 0.5m L6 mol/L mol nitric acid for dissolution and separation;
1.2 chromatographic column preparation
Slowly pouring TBP extraction resin slurry into a quartz chromatographic column filled with deionized water, wherein the inner diameter of the quartz chromatographic column is 6mm, the height of the quartz chromatographic column is 200mm, glass wool is arranged on the bottom of the column, the height of the column is 150mm, the column is uniformly arranged by using a stirring rod, and bubbles are removed by light pressure;
1.3 sample isolation
Transferring the solution to be separated obtained in the step 1.1 into a well-balanced TBP extraction resin chromatographic column, discarding the front 0.3m L effluent liquid, then carrying out leaching by using 8m L6 mol/L nitric acid solution, wherein the leaching speed is 0.4m L/min, receiving the leaching solution into a 10m L quartz volumetric flask, and fixing the volume to the scale by using 6 mol/L nitric acid solution to be used as a solution to be measured;
step 2: instrument preparation
Preheating the ICP spectrometer for more than 60min after starting up, and stabilizing plasma for 15-30 min after ignition;
setting method parameters in software, selecting a silver element analysis spectral line at 328.0nm, and setting the working conditions that the carrier gas flow is 0.5L/min, the RF power is 900W, the sample lifting amount is 1.4L/min, and the auxiliary gas flow is 1.0L/min;
and step 3: drawing working standard curve
Sequentially introducing 6 mol/L nitric acid solution and 1 mu g/m L silver working standard solution into ICP-AES for measurement, and automatically drawing a working standard curve by an instrument;
and 4, step 4: sample assay
Putting the solution to be measured into an ICP spectrometer for measurement, and automatically calculating the concentration value of silver impurity elements by the instrument;
and 5: calculation of results
And (4) repeating the step 1.1, the step 1.3 and the step 4, carrying out 11 blank tests totally, and calculating the content of the silver impurity elements in the MOX pellet sample according to a formula (2).
Figure GDA0002403968830000081
In the formula:
W0i-the content of silver impurity elements in the blank solution, μ g/g;
ρ0i-the concentration value of silver impurity elements in the blank solution, μ g/m L;
v-constant volume of blank solution, m L;
m represents the sample weighing amount and g.
The results of the measurement were as follows:
Figure GDA0002403968830000082
the lower limit of the measurement of the method of the present invention was determined from the first example to be 0.9. mu.g/g, based on the 10-fold standard deviation of the results of 11 blank measurements.
Example two
Step 1: sample processing
1.1 sample dissolution
Grinding MOX pellets into powder with the particle size of less than 150 mu m, weighing 7 parts of 100mg MOX pellet powder to be accurate to 0.0001g, putting 6 parts of the powder into 7 numbered 50m L polytetrafluoroethylene crucibles, and adding 0.1m L10 mu g/m L silver standard solution into 6 parts of the samples;
4m of L concentrated HNO containing 0.1 mol/L of hydrofluoric acid is slowly added into 7 polytetrafluoroethylene crucibles respectively3Dissolving with mixed acid, adding 0.5m L6 mol/L nitric acid solution after the sample is completely dissolved, slowly heating and steaming on an electric furnace until the mixture is nearly dry, and adding 1m L6 mol/L nitric acid solution and H2O2Adjusting the price to 4, heating to drive out H2O2And is concentratedReducing to near dry, adding 0.5m L6 mol/L nitric acid for dissolution and separation;
1.2 chromatographic column preparation
Pouring the TBP extraction resin slurry into a quartz chromatographic column filled with deionized water, wherein the inner diameter of the quartz chromatographic column is 6mm, the height of the quartz chromatographic column is 200mm, glass wool is arranged on the bottom of the quartz chromatographic column, the height of the column is 150mm, the quartz chromatographic column is uniformly arranged by using a stirring rod, bubbles are removed by light pressure, the filled chromatographic column is cleaned by using a 0.1 mol/L nitric acid solution to remove impurities, and then is balanced by using an 8m L6 mol/L nitric acid solution after being washed to be neutral by using deionized water;
1.3 sample isolation
Respectively transferring the solutions to be separated in the step 1.1 into a balanced TBP extraction resin chromatographic column, discarding the front 0.3m L effluent liquid, then carrying out leaching by using 8m L6 mol/L nitric acid solution, wherein the leaching speed is 0.4m L/min, receiving the leaching solution into a 10m L quartz volumetric flask, and carrying out constant volume by using 6 mol/L nitric acid solution to the scale to obtain a sample solution to be measured;
1.4 blank solution preparation
A blank solution was prepared according to steps 1.1-1.3.
Step 2: instrument preparation
Preheating the ICP spectrometer for more than 60min after starting up, and stabilizing plasma for 15-30 min after ignition;
setting method parameters in software, selecting a silver element analysis spectral line at 328.0nm, and setting the working conditions that the carrier gas flow is 0.5L/min, the RF power is 900W, the sample lifting amount is 1.4L/min, and the auxiliary gas flow is 1.0L/min;
and step 3: drawing working standard curve
Sequentially placing 6 mol/L nitric acid solution and 1 mu g/m L silver working standard solution into ICP-AES for measurement, and automatically drawing a working standard curve by an instrument;
and 4, step 4: sample assay
Putting the blank solution and 7 sample solutions to be measured into an ICP spectrometer for measurement, and automatically calculating the concentration value of silver impurity elements by the instrument;
and 5: calculation of results
Calculating the silver content in the MOX core block and the silver content after the addition of the standard according to a formula (1):
Figure GDA0002403968830000101
in the formula:
wi-the content of silver impurity elements in the sample, μ g/g;
ρi-the concentration value of silver impurity element in the sample solution, μ g/m L;
ρ0-the concentration value of silver impurity elements in the blank solution, μ g/m L;
v — volume of sample solution, m L;
m represents the sample weighing amount and g.
The results of the measurement were as follows:
Figure GDA0002403968830000102
Figure GDA0002403968830000111
the results of example two show that: the method for determining the content of the silver impurities in the MOX pellet has the advantages that the standard addition recovery rate is 92-107%, and the measurement precision is superior to 5%.

Claims (9)

1. A method for determining the content of silver impurities in an MOX pellet by adopting TBP extraction resin is characterized by comprising the following steps: the method comprises the following steps:
step 1: sample processing
1.1 sample dissolution
Grinding the MOX pellets into powder with the particle size of less than 150 mu m, weighing 100mg of MOX pellet powder into a polytetrafluoroethylene crucible, and adding 1-4 m L concentrated HNO containing 0.1 mol/L hydrofluoric acid3Dissolving with mixed acid;
after the sample is completely dissolved, 0.5m L6 mol/L nitric acid solution is added, the mixture is slowly heated and steamed on an electric furnace till the mixture is nearly dry, and then 1m L6 mol/L nitric acid solution and H are added2O2Adjusting the valence, after the plutonium is adjusted to 4 valence and the uranium is adjusted to 6 valence, heating to drive out H2O2Concentrating to near dryness, adding 0.5m L6 mol/L mol nitric acid for dissolution and separation;
1.2 chromatographic column preparation
Pouring TBP extraction resin slurry into a quartz chromatographic column filled with deionized water, uniformly loading by using a stirring rod, removing bubbles by light pressure, cleaning the filled chromatographic column by using a 0.1 mol/L nitric acid solution, removing impurities, then washing by using deionized water until the chromatographic column is neutral for later use, and carrying out balance treatment by using a 5-10 m L6 mol/L nitric acid solution before use;
1.3 sample isolation
Transferring the sample solution into a well-balanced TBP extraction resin chromatographic column, then leaching with 7-9 m L6 mol/L nitric acid solution at the leaching speed of 0.2-0.5 m L/min, receiving the leacheate into a 10m L quartz volumetric flask, and fixing the volume to the scale with 6 mol/L nitric acid solution to be used as a solution to be measured;
1.4 blank solution preparation
Preparing a blank solution for the same batch of samples according to the step 1.1-step 1.3;
step 2: instrument preparation
Preheating the ICP spectrometer for more than 60min after starting up, and stabilizing plasma for 15-30 min after ignition;
setting method parameters in software, selecting a silver element analysis spectral line at 328.0nm, and setting the working conditions that the carrier gas flow is 0.5L/min, the RF power is 900W, the sample lifting amount is 1.4L/min, and the auxiliary gas flow is 1.0L/min;
and step 3: drawing working standard curve
Using a 6 mol/L nitric acid solution as a blank standard solution, diluting a silver standard stock solution with the 6 mol/L nitric acid solution to prepare a working standard solution of 1 mu g/m L, introducing the blank standard solution and the working standard solution into an ICP spectrometer in sequence for measurement, and automatically drawing a working standard curve by the instrument;
and 4, step 4: sample assay
The blank solution and the sample solution to be measured are sequentially put into an ICP spectrometer for measurement, and the instrument automatically calculates the blank concentration value rho of the silver impurity element0And sample solution concentration value ρi；
And 5: calculation of results
Calculating the content of silver impurity elements in the MOX pellet sample according to the formula (1):
Figure FDA0002236046390000021
in the formula:
wi-the content of silver impurity elements in the sample, μ g/g;
ρi-the concentration value of silver impurity element in the sample solution, μ g/m L;
ρ0-the concentration value of silver impurity elements in the blank solution, μ g/m L;
v — volume of sample solution, m L;
m represents the sample weighing amount and g.
2. The method for determining the content of silver impurities in the MOX pellet by using the TBP extraction resin as claimed in claim 1, wherein the method comprises the following steps: in the step 1.2, the TBP extraction resin is 150-200 meshes, and 60% of TBP is contained in the TBP extraction resin.
3. The method for determining the content of silver impurities in the MOX pellet by using the TBP extraction resin as claimed in claim 2, wherein the method comprises the following steps: in the step 1.2, the inner diameter of the quartz chromatographic column is 6mm, the height of the quartz chromatographic column is 200mm, the height of the quartz chromatographic column is 150mm, and the bottom of the quartz chromatographic column is filled with glass wool.
4. The method for determining the content of the silver impurities in the MOX pellets by using the TBP extraction resin is characterized in that in the step 1.3, when the sample solution is transferred into a balanced TBP extraction resin chromatographic column, the front 0.3m L effluent is discarded.
5. The method for determining the content of silver impurities in the MOX pellet by using the TBP extraction resin as claimed in claim 4, wherein the method comprises the following steps: and 3, preparing the silver standard stock solution from a certified standard substance GSB G62039-90.
6. The method for determining the content of silver impurities in the MOX pellet by using the TBP extraction resin as claimed in claim 5, wherein the method comprises the following steps: and 5, carrying out data calculation according to GB/T8170 to carry out reduction, wherein the analysis result is less than 10, one decimal is reserved, the analysis result is more than or equal to 10, and the decimal is not reserved.
7. The method for determining the content of silver impurities in the MOX pellet by using the TBP extraction resin as claimed in claim 6, wherein the method comprises the following steps: in step 1, the MOX pellet powder is weighed to be accurate to 0.0001 g.
8. The method for determining the content of silver impurities in the MOX pellet by using the TBP extraction resin as claimed in any one of claims 1 to 7, which is characterized in that: the ICP spectrometer can be in butt joint with the enclosed glove box.
9. The method for determining the content of silver impurities in the MOX pellet by using the TBP extraction resin as claimed in claim 8, wherein the method comprises the following steps: the ICP spectrometer is an IRIS Integrated II type full spectrum direct reading plasma spectrometer produced by ICP-AES, United states thermoelectricity company.
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